Application of solid-phase extraction to determination of polycyclic aromatic hydrocarbons in sewage sludge extracts

doi:10.1016/j.jhazmat.2004.06.015

Journal of Hazardous Materials

Volume 113, Issues 1–3, 10 September 2004, Pages 237-245

https://doi.org/10.1016/j.jhazmat.2004.06.015 Get rights and content

Abstract

The study presents the efficiency of sewage sludge sample clean-up with the application of SPE columns with various types of adsorbents. Six columns were tested: C8-octyl, C18 PolarPlus, C18-octadecyl, silicagel (SG), phenyl, cyano. The highest efficiency of recovery was observed for C18-octadecyl. Then, using C18, the method was optimised by changing the following parameters: eluent type and volume, column drying and effect of washing of cartridge.

Introduction

The most effective way of utilising sewage sludge is its application in agriculture. This method is the preferred method in the European Union countries [1]. Moreover, sewage sludge can be subjected to controlled waste landfill site, incineration and subsequent discharge to the coastal systems [1], [2].

Sewage origin and method of its purification influences the content of various toxic substances, both organic (phenols, polycyclic aromatic hydrocarbons (PAHs), pesticides, polychlorinated biphenyls (PCBs) [3], [4], [5], [6], [7], [8] and inorganic (e.g. heavy metals) [5], [9]. There is a serious danger that a lot of very harmful pollutants (carcinogenic or mutagenic) can be introduced to the soil while fertilising it with sewage sludge [10], [11], [12]. Such pollutants can then undergo various changes in the soil depending on their properties and soil conditions. According to literature [13], pollutants that are very common in sewage sludge belong to the PAH type and are classed as one of the most harmful organic pollutants due to their mutagenic and carcinogenic properties [14], [15].

Soil contamination with PAHs is dangerous as they can get from the soil to plants and then to the further stages of the food chain [16]. It is believed that PAHs get to the human organism mainly with food products.

The cleaning-up of the extracts is a very important step in determination of PAHs in sewage sludge samples. One of the techniques that is widely applied for the purification purposes to get rid of any interferences, is solid-phase extraction (SPE). SPE is a sample treatment technique which passes a liquid sample through a sorbent. The above technique can fulfil two functions. In the first case, the analytes are eluted in a small volume of a solvent and so, the analytes are concentrated; in the second case, the function of the solid-phase extraction is to clean the sample. One of the benefits of using this method is that only small volumes of the solvent are required and the purification time is short. It also allows for a wide variety of extraction conditions which may be used to achieve the desired separation and pre-concentration [17].

C18-octadecyl, C8-octyl, silicagel and florisil are most frequently used for the PAH determination to clean the extracts. Some of the works by other authors [18], [19], [20] quote very good recovery in the case of combining traditional C18 columns with the columns with medium-polar filling such as: amino (NH₂), cyano and phenyl. Some authors [13], [21] gives also information on the immunosorbents (IS) based on the antigen–antibody interactions.

In the studies on the PAH analysis used for the SPE purification [19], [20], [21], [22], [23], there are often contradicting opinions as to the choice of columns and evaluation of their usability. Selection of a purification procedure for specific columns was based on the studies by various researchers [21], [23], [24].

Section snippets

Materials and reagents

Acetonitrile, dichloromethane (DCM), methanol, cyclohexane (CH), n-hexane, tetrahydrofuran (THF) were of the high performance liquid chromatography (HPLC) grade. The standard mixture of PAHs in acetonitrile was obtained from Promochem. The concentration of each analyte was 100 μg/mL. A standard mixture contained 16 EPA priority PAH pollutant: naphthalene (Na), acenaphthylene (Ace), acenaphthene (Ac), fluorene (Fl), phenanthrene (Phen), anthracene (Ant), fluoranthene (Fluo), pyrene (Pyr), benzo[a

Result and discussion

Taking into consideration suggestions by various authors [13], [17], [19], [21], [26], [27], process optimisation was based on the following criteria: choice of columns, selection of the eluent, effect of the eluent volume, column drying before PAH elution, effect of washing cartridge.

Conclusions

The preliminary studies with the view of selecting an appropriate column for further optimisation processes showed that the highest recovery rate (88%) with a simultaneous high reproducibility (R.S.D. = 3–9%, only naphthalene = 13%) was achieved on the columns with octadecyl filling C18. Also on the C18 PP columns, reproducibility was high (R.S.D. = 3–11%).

Optimisation of the individual phases of the processes influenced mainly the changes in the recovery of low molecular weight (LMW) PAHs

Acknowledgements

Financial support from the State Committee for Scientific Research (KBN, Warsaw, Poland), project No. P06H 06220 is gratefully acknowledged. P. Oleszczuk is granted by the Foundation for Polish Science.

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Application of solid-phase extraction to determination of polycyclic aromatic hydrocarbons in sewage sludge extracts

Abstract

Introduction

Section snippets

Materials and reagents

Result and discussion

Conclusions

Acknowledgements

Sci. Total Environ.

Sci. Total Environ.

J. Chromatogr. A

J. Chromatogr. A

Chemosphere

J. Chromatogr. A

Geoderma

J. Chromatogr. A

Anal. Chim. Acta

J. Chromatogr. A

J. Chromatogr. A

J. Chromatogr. A

J. Chromatogr. A

J. Chromatogr. A

Commun. Soil Sci. Plant Anal.

J. Environ. Qual.

Pol. J. Environ. Stud.